血样和尿样中毒鼠强气相色谱测定方法的研究及其初步应用

〕本文报道一种血、尿样品里毒鼠强的分离与分析方法。血样加入10W/VNaCl用乙酸乙酯萃取,尿样以X5树脂小柱固相萃取,气相色谱测定。所建方法已用于1例中毒病人血、尿样品的测定,在中毒4天后血中、7天后尿中仍可测出毒鼠强。另外,本方法还用于对治疗该病人的人工炭肾内毒鼠强的测定,根据测定结果对人工炭肾的疗效进行了评价。     

DEIP中微量杂质的GC/MS分析

研究了间苯二甲酸二乙酯(DEIP)中微量杂质的化学成分,用减压精馏的方法对样品进行分离浓缩,用气相色谱-质谱法(GC/MS)进行分析,结合生产工艺,谱库检索及人工解谱进行鉴定,鉴定出DEIP中主要11种杂质,用归一化法进行定量,建立了用GC/MS方法检测DEIP中微量杂质的方法。     

生物检材中液化石油气成份的分析

近年来,可疑液化石油气(和天然气)中毒死亡的案件时有发生.该种案件的发生不随季节变化,春夏秋冬都有利用其作为自杀或杀人手段的.本文研究用顶空-GC-MS法对中毒血液中液化气主要成份进行简便易行的分离、鉴定.液化石油气的成份是C5以下的低炭烃类,主要是C3～C 5的烷烃、烯烃,以C4居多.     

中药党参挥发性成分分析

采用“乙醚冷浸－索氏提取－水蒸汽蒸馏”方法对党参中挥发性成分进行提取,用ＧＣ分离,加标定性和ＧＣ－ＭＳ联用鉴定其组分。分离出２６８种化合物,鉴定出６４种。     

江西猪油中毒事件中有机锡形态的研究

本文利用气相色谱-火焰光度(GC-FPD)、气相色谱-质谱联用(GC-MS)和等离子体-质谱(ICP-MS)等检测技术对1999年元旦期间发生在江西赣州龙南、定南两县猪油中毒事件中的污染油样,中毒病人的尿样、血样以及中毒死者内脏中的有机锡形态进行了综合研究,并得出了明确结论.认为三甲基锡和二甲基锡是造成这次罕见事件的主要中毒成分,同时还发现一甲基锡、二辛基锡、无机锡和其它重金属污染物的存在.     

液相色谱-串联质谱法鉴定大鼠血浆中的东莨菪碱及其代谢物

建立了鉴别东莨菪碱及其代谢物的液相色谱-电喷雾离子阱串联质谱(LC-MSn)联用方法。取单剂量灌胃50 mg/kg东莨菪碱的大鼠血样,甲醇沉淀蛋白,采用LC-MS及LC-MSn等方法分析血样。和空白血样及东莨菪碱相比较,根据血样中代谢物分子量的变化(ΔM)及其多级质谱数据,鉴定并阐述其结构。结果在服药后的大鼠血样中发现7种代谢物,分别为莨菪品、N-去甲基莨菪品、脱水东莨菪碱,N-去甲基脱水东莨菪碱、N-去甲基东莨菪碱、氧化东莨菪碱以及托品酸等。该方法灵敏,快速,简便,适合于药物及其代谢物的快速鉴定。     

江西猪油中毒事件中的有机锡形态

利用气相色谱－火焰光度（ＧＣ－ＦＰＤ）、气相色谱－质谱联用（ＧＣ－ＭＳ）和等离子体－质谱（ＩＣＰ－ＭＳ）等检测技术对１９９９年元旦期间发生在江西赣州龙南、定南两县猪油中毒事件中的污染油样,中毒病人的尿样、血样以及中毒死者内脏中的有机锡形态进行了综合研究,并得出了明确结论．认为三甲基锡和二甲基锡是造成这次罕见事件的主要中毒成分,同时还发现一甲基锡、二辛基锡、无机锡和其他重金属污染物的存在．     

气相色谱-质谱法同时筛检人血液中26种常见毒药物

建立了气相色谱-质谱法(GC-MS)同时快速筛检人血液中26种常见毒药物的新方法.通过对样品前处理方法的摸索及GC-MS分析条件的优化,采用磷酸盐缓冲液(pH 3.5)稀释血样后,乙醚萃取,分段选择离子监测(SIM)法鉴定,并用提取离子进一步验证,可以同时检测甲胺磷、毒鼠强、地西泮、尼可刹米、利多卡因、苯巴比妥、阿托品等7大类共26种常见毒药物,回收率大部分达80%～90%,检测限为0.01 mg/L.本法用色谱保留时间、质谱特征离子同时定性,消除了血液中复杂基体的干扰,适用于中毒患者血液的应急检测.     

剌梨利康饮对汞中毒大鼠汞铜锌含量的影响

用高汞水喂养大鼠８周,复制出慢性汞中毒模型,再分别自由饮用利康饮饮料和腹腔注射二巯基丙磺酸钠３周,探讨剌梨利康饮和二巯基丙磺酸钠对慢性汞中毒大鼠体内汞、铜、锌含量的影响。结果显示：慢性汞中毒引起血清、肝、脑和肾中汞含量升高的同时,引起血清、脑和肾中铜、锌含量及肝中锌含量降低;利康饮可降低血清和肾中汞含量,并可提高血清、脑和肾中铜、锌含量及肝含量;二巯基丙磺酸钠虽可降低血清、肝和肾中汞含量,升高血清     

刺梨利康饮对汞中毒大鼠汞铜锌含量的影响

用高汞水喂养大鼠8周,复制出慢性汞中毒模型,再分别自由饮用利康饮饮料和腹腔注射二巯基丙磺酸钠3周,探讨刺梨利康饮和二巯基丙磺酸钠对慢性汞中毒大鼠体内汞、铜、锌含量的影响.结果显示:慢性汞中毒引起血清、肝、脑和肾中汞含量升高的同时,引起血清、脑和肾中铜、锌含量及肝中锌含量降低;利康饮可降低血清和肾中汞含量,并可提高血清、脑和肾中铜、锌含量及肝中锌含量;二巯基丙磺酸钠虽可降低血清、肝和肾中汞含量,升高血清和肾中铜含量,但引起血清和肝中锌含量更加降低.结果表明:利康饮可降低慢性汞中毒大鼠体内汞的负荷量,并具有补充铜、锌微量元素的作用.     

O,O,S-三甲基硫赶磷酸酯在甲胺磷中毒检验中的应用

利用气相色诤质谱(GC-MS)分析了甲胺磷中毒者的检材(血，胃内容物)，均检出了O，O，S-三甲基硫赶磷酸酯，确未检出过甲胺磷。研究了这一现象的原因和确定了O，O，S-三甲基硫赶磷酸酯(O，O，S-TMTP)可作为甲胺磷中毒的佐证物。     

二十六种滥用药物的气相色谱及气相色谱－质谱系统分析方法的研究

建立了二十六种滥用药物的分离和分析方法。利用气相色谱（ＧＣ）分离和质谱（ＭＳ）差谱技术，二十六种药物都得到有效地分离和检测。此法被证明对中毒者的生物样品进行滥用药物及其代谢物的检测和鉴定是重要的和有效的。     

A De Novo Designed Metalloenzyme for the Hydration of CO2

Protein design will ultimately allow for the creation of artificial enzymes with novel functions and unprecedented stability. To test our current mastery of nature’s approach to catalysis, a Zn^II metalloenzyme was prepared using de novo design. α₃DH₃ folds into a stable single‐stranded three‐helix bundle and binds Zn^II with high affinity using His₃O coordination. The resulting metalloenzyme catalyzes the hydration of CO₂ better than any small molecule model of carbonic anhydrase and with an efficiency within 1400‐fold of the fastest carbonic anhydrase isoform, CAII, and 11‐fold of CAIII.     

Permselectivity Replication of Artificial Glomerular Basement Membranes in Nanoporous Collagen Multilayers

Basement membranes (BMs) play important roles in many biological functions such as tissue regeneration, cancer proliferation, nutrient/drug delivery, breathing, and many others. While there are many theoretical models, adequate experimental analogs of BMs describing basic physicochemical properties of BM, such as diffusion and permselectivity are not available. Taking BMs found in glomerulus of kidneys as an example, adequate reproduction of their permselectivity requires biomimetic membranes with submicron thickness, high uniformity, nanoscale porosity, and size-selective permeability. Artificial kidney BMs were assembled from poly(acrylic acid) and collagen using layer-by-layer (LBL) assembly technology and display multiple structural similarities with glomerular BMs. Diffusional transport through the artificial BMs faithfully replicate cut-off parameters of kidney membranes. Their utilization in understanding of unique diffusion processes in kidneys, in vitro studies of blood clearance time of small drugs/nanoscale drug carriers and design of more complex organoids including live cells for cancer proliferation studies is anticipated.     

A carbonic anhydrase inhibitor induces bicarbonate-reversible suppression of electron transfer in pea photosystem 2 membrane fragments

The effects of suppression of the carbonic anhydrase (CA) activity by a CA-inhibitor, acetazolamide (AA), on the photosynthetic activities of photosystem II (PS II) particles from higher plants were investigated. AA along with CA-activity inhibits the PS II photosynthetic electron transfer and the AA-induced suppression is totally reversed by the addition of bicarbonate (3-5 mM). Similar effect of recovery in the PS II photosynthetic activity was also revealed upon the addition of known artificial electron donors (potassium ferrocyanide and TMPD). Significance and possible functions of CA for the PS II donor side are discussed.     

Influence on elemental status by hip-endoprostheses

For many clinical purposes various artificial devices are applied, which contact human tissue and can thus cause adverse reactions between prosthetic surfaces and body components. Of the many materials applied for orthopaedic joint replacements the most common are cobalt-chromium-molybdenum alloys. In these cases considerable amounts of cobalt-chromium-molybdenum wear particles are released from the prostheses which have to be regarded as a cause of long-time problems for the patient.Since these particles are dissolved in body fluids of the surrounding area they are distributed in the whole body via blood. Elevated metal concentrations have been found in blood and urine of persons with endoprostheses. Partly the metals are excreted via urine, but to some extend they accumulate in different organs.Therefore this study dealt with the development of an analytical method for the determination of seven relevant trace elements, namely Al, Co, Cr, Mo, Nb, Ni, and Ti in nine kinds of human tissue (brain, heart, kidney, liver, lung, muscle, lymphatic nodes, spleen, body fat) starting with drawing of the sample, sample work up and finally analysis by means of atomic spectrometry. The optimized method was then applied to determine the metal contents in organs of persons (post mortem) with total hip replacements with metal on metal bearing surfaces. Comparison of the data obtained with those of persons without hip-endoprostheses shows that brain and lung are the main targets for elemental accumulation in persons with hip-endoprostheses. Mo and Nb represent the elements with the highest tendency to be accumulated.     

轻度铅中毒对儿童微量元素及骨龄的影响

为探讨儿童轻度铅中毒对微量元素及骨龄的影响,采用钨舟原子化法和原子吸收光谱法分别检测了33例轻度铅中毒患儿血铅及微量元素水平,用X摄片进行骨龄测定,并进行了相关分析。结果表明,轻度铅中毒患儿微量元素钙、铁、锌降低,骨龄发育落后,血铅含量与钙、铁、锌水平呈负相关。提示轻度铅中毒使儿童骨龄落后,可能与微量元素间的失衡有关。     

中毒患者血清和尿液中毒鼠强残留物的GC-MS分析方法

有关资料表明,人和动物口服毒鼠强后,其血液、尿液和各脏器中均有毒鼠强残留物出现,残留时间从药后数小时至几天乃至十几天之内不等。可见血液和尿液作为可印证中毒病人中毒原因的直接样品更值得我们去关注,与呕吐物、可疑食物等检品相比,它具有提取相对简单,干扰成分少,残留时间长以及可反复采集等许多优点。因此,我们结合突发性中毒检验工作的需要,利用超声波液-液萃取技术,研究了中毒患者血清和尿液中毒鼠强残留物的GC-MS-SIM检测方法。在对40多人份血清和尿液添加标准物的反复测定中,回收率血清保持在90.8％～99.5％;RSD为3.82％,尿液保持在91.2％～102.8％,RSD为4.91％,全过程仅需约30min。经过两年来百多份样品检测的验证,该方法不失为日常快速分析中毒患者血清和尿液中毒鼠强残留物的一种有效方法,现介绍如下。     

脲和盐酸胍诱导的牛碳酸酐酶B的去折叠

采用非变性聚丙烯酰胺凝胶电泳、十二烷基硫酸钠-聚丙烯酰胺凝胶电泳、高效凝胶排阻色谱和激光光散射光谱研究了脲和盐酸胍诱导的牛碳酸酐酶B的去折叠.实验结果表明,在脲和盐酸胍诱导的牛碳酸酐酶B的去折叠过程中,溶液中只含有单分子牛碳酸酐酶B和二分子牛碳酸酐酶B集聚体;二分子牛碳酸酐酶B集聚体是通过单分子牛碳酸酐酶B之间的疏水和...     

离子排斥色谱法测定甘油催化氧化产物中的H2CO3和HCOOH

建立了测定甘油催化氧化产物中H2CO3和HCOOH的离子排斥色谱分析方法。采用离子排斥柱分离,分别用纯水和4 mmol/L HCl作流动相进行H2CO3和HCOOH的分析。检测方式为非抑制电导检测。实验结果显示,H2CO3和HCOOH工作曲线的线性范围为2～100 mg/L和6.23～124.6 mg/L,检出限分别为0.45 mg/L和2.49 mg/L(S/N=3)。H2CO3的保留时间和峰面积的相对标准偏差分别为0.07%和4.0%,HCOOH的保留时间和峰面积的相对标准偏差分别为0.09%和2.2%。方法已用于甘油催化氧化产物中H2CO3和HCOOH的分析。